Diethyl Ether → 4-{[(1S,2R)-2-aminocyclohexyl]amino}-N-(2-methoxyethyl)-6-methylquinazolin-2-carboxamide

HRID 1971135ノート

反応式

HRID 1971135 の反応式
C(OC(=O)[NH:7][C@@H:8]1[CH2:13][CH2:12][CH2:11][CH2:10][C@@H:9]1[NH:14][C:15]1[C:24]2[C:19](=[CH:20][CH:21]=[C:22]([CH3:25])[CH:23]=2)[N:18]=[C:17]([C:26]([NH:28][CH2:29][CH2:30][O:31][CH3:32])=[O:27])[N:16]=1)(C)(C)C.C(OCC)(=O)C.Cl.C(OCC)C>C(OCC)(=O)C>[NH2:7][C@@H:8]1[CH2:13][CH2:12][CH2:11][CH2:10][C@@H:9]1[NH:14][C:15]1[C:24]2[C:19](=[CH:20][CH:21]=[C:22]([CH3:25])[CH:23]=2)[N:18]=[C:17]([C:26]([NH:28][CH2:29][CH2:30][O:31][CH3:32])=[O:27])[N:16]=1

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 21866389Hydrogen chloride-ethyl acetateHCID 86638400tert-butyl {(1R,2S)-2-[(2-{[(2-methoxyethyl)amino]carbonyl}-6-methylquinazolin-4-yl)amino]cyclohexyl}carbamate

生成物 1

HCID 687002114-{[(1S,2R)-2-aminocyclohexyl]amino}-N-(2-methoxyethyl)-6-methylquinazolin-2-carboxamide収率 92%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a suspension of 2.24 g of tert-butyl{(1R,2S)-2-[(2-{[(2-methoxyethyl)amino]carbonyl}-6-methylquinazolin-4-yl)amino]cyclohexyl}carbamate in 10 ml of ethyl acetate, 10 ml of a 4 N hydrogen chloride-ethyl acetate solution was added, and the mixture was stirred at room temperature for 48 hours. To the reaction solution, 20 ml of diethyl ether was added, and the mixture was stirred for 30 minutes. Then, the deposited substance was collected by filtration, washed with diethyl ether and dried under reduced pressure. The resulting powder was purified by Fuji Silysia NH silica gel column chromatography (chloroform:methanol=20:1), whereby 1.61 g of a desired compound was obtained as a colorless powder.

後処理

  1. additionwas added
  2. stirringthe mixture was stirred for 30 minutes
  3. filtrationThen, the deposited substance was collected by filtration
  4. washwashed with diethyl ether
  5. customdried under reduced pressure
  6. customThe resulting powder was purified by Fuji Silysia NH silica gel column chromatography (chloroform:methanol=20:1)

出典と根拠

ORDレコード
ord-cac9a387d8bc4b87be7c978704ff41db
出典データセット
uspto-grants-2013_04
特許番号
US08431586B2

反応ノート

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